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A kind of phase-transfer catalytic interfacial polycondensation method preparation and separation and purification method of polyarylate

A purification method and polyarylate technology are applied in the field of preparation of copolyarylate resin to achieve the effects of low consumption, simplified process and reduced production cost

Active Publication Date: 2016-04-06
JIANGYIN BOSHENG NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through aroyl dichloride and bisphenol monomers of different structures, various new varieties of copolyarylates with different properties have been synthesized. There are few detailed reports on issues such as resin thermo-oxidative stability and manufacturing cost.

Method used

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  • A kind of phase-transfer catalytic interfacial polycondensation method preparation and separation and purification method of polyarylate
  • A kind of phase-transfer catalytic interfacial polycondensation method preparation and separation and purification method of polyarylate
  • A kind of phase-transfer catalytic interfacial polycondensation method preparation and separation and purification method of polyarylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The typical preparation process of PAR resin refining solution is as follows:

[0035] Add 500 mL of deionized water, 0.3 g of sodium bisulfite, and 26.4 g (0.66 mol) of sodium hydroxide into a clean 3000 mL three-necked flask equipped with an electric stirrer. 68.4g (0.30mol) of bisphenol A, stir to completely dissolve bisphenol A to form a water-soluble sodium salt, add 0.50-1.0g of benzyltriethylamine chloride, stir and cool to below 10°C.

[0036] Dissolve 18.64g (0.0918mol) of TPC and 43.48g (0.2142mol) of IPC in 1000mL of dichloroethane to form an organic phase. Slowly add the organic phase to the above-prepared aqueous phase under rapid stirring, and complete the addition in about 30 minutes. Then add 50 mL of aqueous solution containing 1.18 g (0.0126 mol) of phenol and 0.53 g (0.013 mol) of NaOH, continue stirring for about 4 hours, neutralize the excess NaOH in the reaction liquid with formic acid, and make the pH value of the reaction mixture to 3-5 , static...

Embodiment 2

[0045] With the reclaimed methylene chloride (37 ℃~41 ℃ fraction), prepare PAR resin according to the same operation procedure of embodiment 1, experimental result is listed in table 2.

[0046] Table 2 reclaims dichloromethane to PAR resin η inh Impact

[0047]

[0048] *Dichloromethane and THF are the experimental data of the first use of industrial products; 2~6 are the data of recovery of dichloromethane and THF. Example 3

Embodiment 3

[0049] Use 1,2-ethylene dichloride instead as the organic phase solvent, and DMF is as the separating agent, and according to the method of embodiment 1, the η of PAR resin inh 1 is 0.67dL / g, and the DMF separating agent is evaporated to obtain white granular resin, η inh 2=0.71dL / g, after heating and melting at 300℃±10℃ for 5min, the resin is colorless and transparent, η inh 3 is 0.68dL / g, Δη inh =-0.03dL / g, the resin yield was 94.4%.

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Abstract

The invention discloses a method for preparing and purifying polyarylester (PAR) as shown in a formula. The method is characterized in that the resin separation, grinding and purification and the solvent recovery are realized by adopting a one-step process in a resin dichloromethane solution of PAR prepared by adopting a phase-transfer catalysis interface polycondensation process. A recovered solvent can be directly recycled without being rectified. The thermal oxidation stability of prepared PAR resin is improved, and melting requirements can be met.

Description

Technical field: [0001] The present invention relates to the preparation of copolyarylate (PAR) resin. technical background: [0002] The phase transfer catalytic interfacial polycondensation method uses water and water-immiscible organic solvents as the medium, and two or more polymerizable monomers are respectively dissolved in the aqueous phase and the organic phase. Under the action of rapid stirring and shearing force, the polycondensation reaction It proceeds quickly at the two-phase interface. After the polycondensation reaction is completed, the resin is generally dissolved in the organic phase. After washing with deionized water to remove salt and impurities, the refined resin glue is obtained. According to the process of isolating the resin from the fine glue, it is different. , Divided into precipitation method, vaporization method and thin film evaporation method. The interfacial polycondensation method is an irreversible process carried out in a heterogeneous p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/20C08G63/195C08G63/197C08G63/183C08G63/181C08G63/79C08G63/90C08J11/02
Inventor 宋才生任华平
Owner JIANGYIN BOSHENG NEW MATERIAL TECH
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